RU2503181C1 - Method of production of biologically active preparation based on alfalfa - Google Patents

Abstract

FIELD: agriculture.

SUBSTANCE: invention relates to the field of agriculture and can be used as a bio-stimulator to improve the growth, development and productivity of plants. The method of production of biologically active preparation based on alfalfa hay comprises steaming the hay in the water condensate at a temperature up to 100°C and a weight ratio of plant materials to condensate of 1:11, the introduction of micro-and macroelements in the form of an aqueous solution of metal salts to obtain enriched suspension of hay, carrying out high-temperature hydrolysis of enriched suspension of hay at a temperature of 150-160°C and a pressure of 4.5-6 atm for 40-90 minutes to obtain a concentrated hydrolyzate and its purification from wastes. The method provides a multiple recycle of the concentrated purified hydrolyzate at the stage of steaming the alfalfa hay, at that at every stage of recycle the loading with new hay portion, water condensation and micro- and macroelements is carried out to the steaming unit. The weight of the newly loaded hay, water condensation and micro- and macroelements is equivalent to weight of waste. When the concentration of nutrients in the concentrated hydrolyzate is more than 5% the part of the concentrated hydrolyzate is directed to evaporation at a temperature of 60-120°C to obtain a concentrated product - a biologically active preparation in which the concentration of biologically active substances is 38.5-41.5%.

EFFECT: proposed method enables to increase the productivity of the process and to obtain a preparation with a higher content of biologically active substances.

3 cl, 2 tbl, 1 dwg, 1 ex

Description

The invention relates to the field of agriculture and can be used as a biostimulant to improve the growth, development and increase of plant productivity.

A known method of obtaining a biologically active drug based on alfalfa extract [patent No. 2145863, IPC A61K 35/78, publ. 02/27/2000), including treatment of plant materials with an extractant containing an aqueous solution of salts, exposure of the extracting mixture at a temperature of 150 ° C and elevated pressure, separation, purification and drying of the extract, processing of alfalfa or hay of alfalfa is carried out with a mixture of aqueous solutions of trace elements Ba, Sn, Co , Cr, V, Zn, Fe, Se, Mn, Cu, moreover, the ratio of the crushed plant material to the extractant is 1: 8. The processing of plant materials with an extractant is carried out at a temperature of 60-80 ° C with stirring for 20 minutes The extract is dried at a temperature of 200-300 ° C. In addition, the extracting mixture was incubated for 90 minutes at a pressure of 5.4-5.9105 Pa.

Significant disadvantages of the method is the use in the formulation of a small amount of alfalfa hay 12.5 wt.% Or in the ratio of plant materials: extractant 1: 8, and the temperature of extraction of 140-150 ° C, the extraction time of 90 minutes which is not enough for bioflavonoids to exit from alfalfa to the extract. Thus, the technological regimes used and the recipe lead to a low concentration of biologically active substances, in particular flavonoids, in the resulting BAP.

Also known is a method of obtaining biologically active additives "Eramin" [patent No. 2435455, IPC A23L 1/30, publ. 12/10/2011], including the preparation of plant materials, weighing the components of the formulation, the preparation of a solution from a dry mixture of alfalfa hay, trace elements and distilled water, extraction in time at a pressure of 6 × 105 Pa, drying of the extract in an oven at a temperature of 55-60 ° C for a duration 4 hours. According to the invention, a solution is prepared from a dry mixture of alfalfa hay and trace elements with alfalfa hay content of at least 40-60 wt.%, Extracted at a temperature of 180-190 ° C for 5-6 hours.

A significant drawback of this process is the high temperature of hydrolysis, at which part of the nutrients are disrupted and tarred. The process of hydrolysis of plant materials partially coincides with the formation of the product, while a significant part of the operations is performed manually, which leads to low productivity of the method and a significant cost overrun of raw materials and energy costs.

The closest is a method of obtaining a biologically active drug [patent No. 2335925, class. A23L 1/30, A23L 1/304, A23L 1/305, A23L 1/302, A61K 36/00, publ. 10.20.2008]. A method of obtaining a biologically active drug based on alfalfa, including grinding vegetable raw materials, processing it with an extractant containing an aqueous solution of salts of macro- and micronutrients, holding the extracting mixture at elevated temperature and elevated pressure, with further separation, purification and drying of the obtained extract, first extraction of plant materials with condensate heated to a temperature of 60-80 ° C for 0.3-0.5 hours, while the ratio of condensate to plant materials is 6: 1 wt., gave part of the extract is transferred to an intermediate tank, and the rest is fed to “hot extraction” in a steam-heated apparatus into which aqueous solutions of macro- and microelements are introduced per 1 kg of plant material, and “hot extraction” is carried out at a temperature of 110 -140 ° C and a pressure of 1.5-4.5 atm for 0.6-1.2 hours, after which the excess pressure is released, and the temperature is reduced to 100 ° C, and at this temperature the mixture can withstand another 0.2- 0.8 h, then the resulting extract is fed to filtration and evaporation, where evaporation takes place e to a concentration of 45-50%, after which one stripped off the extract is combined with a cold extract, while the mass ratio of the cold extract to one stripped off is 4.0-6.0: 36.0, and then the finished mixture is served for bottling or freeze-drying and further to the packaging.

Significant disadvantages of this method is the use in the formulation of a small amount of alfalfa hay 6 wt.% Or in the ratio of plant materials: extractant 1: 6, and the temperature of extraction of 110-140 ° C, the extraction time of 90 minutes which is not enough for bioflavonoids to exit from alfalfa to the extract. Thus, the used technological regimes and the formulation leads to a low concentration of biologically active substances, in particular flavonoids in the resulting BAP.

The technical task of the alleged invention is the development of a method for producing a biologically active preparation based on alfalfa hay, having a high content of biologically active substances and an increase in the productivity of the process.

The problem is solved in that the proposed method for producing a biologically active preparation based on alfalfa hay involves haying in water condensate at a temperature of up to 100 ° C and a mass ratio of plant materials to condensate of 1:11, the division of micro and macro elements in the form of an aqueous solution of salts metals to obtain an enriched suspension of hay, high-temperature hydrolysis of an enriched suspension of hay at a temperature of 150-160 ° C and a pressure of 4.5-6 atm for 40-90 minutes to obtain a concentrated hydrolyzate, many multiple recycle of the concentrated hydrolyzate, wherein at each stage recycle hay are downloading new portion of condensed water and micro- and macroelements park the unit and cleaning waste from the concentrated hydrolyzate. The mass of newly loaded hay, water condensate and micro and macro elements should be equivalent to the mass of waste. Upon reaching a nutrient concentration of more than 5% in the concentrated hydrolyzate, part of the concentrated hydrolyzate is sent to evaporation at a temperature of 60-120 ° C to obtain a concentrated product - the desired biologically active preparation, in which the concentration of biologically active substances is 38.5-41.5%, at the same time, an equivalent amount of aqueous condensate and micro and macro elements are added to the hay parker.

The introduction of micro and macro elements is carried out at the stage of hay steaming in water condensate in the following ratio, mg / kg of plant material:

iron sulfate 7-water - 0.450-650 zinc sulfate 7-water 0.13-0.17 5-manganese sulfate 0.065-0.89 5-hydrous copper sulfate 0.001-0.004 ammonium vanadium 0.006-0.007 cobalt sulfate 7-water 0.015-0.017 chlorine tin 0.015-0.017 barium chloride 0.005-0.006 selenium 0.001-0.003

Obtaining a product with increased biological activity is provided by the proposed sequence, namely the steaming process, high-temperature hydrolysis of a hay suspension to obtain a concentrated hydrolyzate, repeated recycle of the concentrated hydrolyzate, the formation of a biologically active preparation at a reduced temperature at the evaporation stage.

Zaparki with water condensate allows partial extraction of biologically active substances of alfalfa in the resulting suspension of hay. Hydrolysis at elevated temperatures can reduce the process time to an interval of 40-90 minutes, and enrichment as a result of recycling the initial hay suspension allows you to get a highly concentrated biologically active drug based on alfalfa hay.

During high-temperature hydrolysis, nutrients are extracted from seed alfalfa in the form of water-soluble compounds, which are chelate aggregates obtained from organic substances (from monosaccharides, disaccharides, glucosides from a number of saponins, thioglucosides, pectin - cellulose compounds, protein compounds) and macro- and microelements (iron, pink, calcium, phosphorus, magnesium, manganese, sulfur, potassium, silicon, fluorine, tin, vanadium and barium). During the hydrolysis of a hay suspension, organic compounds are formed that are tightly bound to metal ions. An aqueous extract of chelating compounds is able to form a condensed extract in which multivitamin complexes, essential amino acids, flavanoids, uronic acids are formed.

The proposed method is illustrated by the circuit shown in Fig. 1. Where

1 - block hay parking,

2 - block high-temperature hydrolysis of an enriched suspension of hay,

3 - residue block,

4 - block receiving the finished product

5 - block cleaning concentrated hydrolyzate,

I is the feed line,

II - feed line enriched suspension of hay,

III - feed line of concentrated hydrolyzate,

IV - feed line of concentrated hydrolyzate with solid waste,

V is the feed line of the purified concentrated hydrolyzate,

VI - waste disposal line,

VII - feed line of the finished product,

VIII - the supply line of micro and macro elements in the form of an aqueous solution of metal salts,

IX - water condensate feed line,

The feedstock, crushed alfalfa hay, is fed through line I to block 1 for steaming in water condensate at temperatures up to 100 ° C and a mass ratio of plant material to condensate of 1:11. Along lines IX and VIII, water condensate with a temperature of up to 100 ° C and micro and macro elements in the form of an aqueous solution of metal salts are introduced into block 1 to obtain an enriched suspension of hay. Line II enriched slurry of hay fed fiber 2, which produces high-temperature hydrolysis.

In the first stage of recycle by Liplin IV from the high-temperature hydrolysis unit 2, the concentrated hydrolyzate containing waste is discharged and fed to the unit 4 for purification. Via line V, the purified concentrated hydrolyzate is fed to block 1 to prepare the next portion of the hay suspension. At the same time, a new portion of hay, water condensate, and micro and macro elements is fed into block 1. Line VI discharges waste from block 4.

In the subsequent stages of the recycle, all operations are repeated. On the block of high-temperature hydrolysis, the concentration of nutrients in the concentrated hydrolyzate is constantly monitored.

Upon reaching the concentration of nutrients in the concentrated hydrolyzate of more than 5%, a part of the concentrated hydrolyzate along line III is sent to block 3 for evaporation to obtain a concentrated biologically active preparation, from where it is removed through line VII.

The invention is illustrated by examples:

Example 1. In block 1 is loaded with 50 kg of hay and 500 l of water condensate with micro and macro elements.

In a block 2, which is a steel reactor made of X18H10T steel with a volume of 1000 l, equipped with a bubbler for supplying steam into the reactor and an external steam jacket for supplying steam by the deaf method, a hay suspension prepared in 1 block is fed. Hydrolysis is carried out at a temperature of 50 degrees, at atmospheric pressure. The resulting product was subjected to analysis. The results are listed in table 1.

The following examples 2-10 were carried out at a temperature of from 100 degrees and above, and at a pressure of atmospheric to 6 atm. The results are summarized in tables 1 and 2.

Table 1. The concentration of nutrients in the concentrated hydrolyzate obtained by a single recycling No. t ° C R atm Suspension of hay with water condensate and trace elements kg / operation Hydrolysis time in min Concentrated Hydrolyzate, g / l Note one fifty atm Hay 50 kg. Water condensate with micro and macro elements 500 l. 90 Hydrolysis does not go 2 one hundred atm Hay 50 kg. Water condensate with micro and macro elements 500 l. 90 Hydrolysis does not go 3 115 1,5 Hay 50 kg. Water condensate with micro and macro elements 500 l. 90 0.1 Hydrolysis does not go four 125 2,5 Hay 50 kg. Water condensate with micro and macro elements 500 l. 90 0, .3 Product yield 0.5%, nutrient recovery 4.5% 5 140 4.0 Hay 50 kg. Water condensate with micro and macro elements 500 l. 90 1,5 Product yield 7.4%; nutrient recovery 66.66% 6 150 5.5 Hay 50 kg. Water condensate with micro and macro elements 500 l. 90 2,3 Product yield 10.1%; nutrient recovery 90.9% 7 160 5.9 Hay 50 kg. Water condensate with micro and macro elements 500 l. 90 2.45 Product yield 10.9%, nutrient recovery 98.19% 8 170 6.4 Hay 50 kg. Water condensate with micro and macro elements 500 l. 90 2.45 Product yield 10.9%, nutrient recovery 98.19% Raising the temperature above 160 ° C is not advisable, because nutrients extracted completely. 9 160 5.9 Hay 50 kg. Water condensate with micro and macro elements 500 l. 60 2.45 Product yield 10.9%, nutrient recovery 98.19% 10 160 5.9 Hay 50 kg. Water condensate with micro and macro elements 500 l. 40 2.35 Product yield 10.0%, nutrient recovery 90.1%

Conducting multiple recycling in order to increase the concentration of nutrients in the finished product is advisable at a temperature of 150-160 ° C and a pressure of 4.5-6 atm for 40-90 minutes.

Table 2. Increasing the concentration of nutrients as a result of triple recycling (example 7) No. t ° C P ati Suspension of hay with water condensate and trace elements kg / operation Hydrolysis time in min Concentrated Hydrolyzate, g / l Note one 160 5.9 Hay 50 kg. Water condensate with micro and macro elements 500 l. 90 2.45 Product yield 10.9%, nutrient recovery 98.19% 2 160 5.9 Hay 50 kg. Water hydrolyzate (recycle containing 2.45 g / l of nutrients) 90 4.2 Product yield 21.8%; nutrient recovery 90.19% 3 160 5.9 Hay 50 kg. Water hydrolyzate (recycle containing 4.2 g / l of nutrients) 90 7.9 Product yield 39.4%; nutrient recovery 98.19%

The proposed method allows to increase the specific productivity of technological equipment, by repeated recirculation of the hydrolyzate and the technological chain, to obtain a product with high biological activity. Resin formation is less likely to occur in the product, and under gentle conditions the formation of the product is less likely to destroy the active part of the biologically active drug. An increase in the concentration of nutrients sharply reduces energy consumption and doubles the productivity of removing the product from a unit volume of technological equipment.

Claims (3)

1. A method of producing a biologically active preparation based on alfalfa hay, including hay stocking in an aqueous condensate, introducing micro and macro elements in the form of an aqueous solution of metal salts to obtain an enriched suspension of hay, conducting high-temperature hydrolysis of an enriched suspension of hay to obtain a concentrated hydrolyzate, forming a biologically active preparation at a reduced temperature at the stage of evaporation, characterized in that the method further includes repeated recycling of concentrated gy rolizata, park the hay in the aqueous condensate is conducted at a temperature up to 100 ° C and a weight ratio of plant raw material to condensate 1:11 introduction of micro- and macroelements produced in the following ratio, mg / kg of vegetable raw materials:
iron sulfate 7-water 0.450-650 zinc sulfate 7-water 0.13-0.17 5-manganese sulfate 0.065-0.89 5-hydrous copper sulfate 0.001-0.004 ammonium vanadium 0.006-0.007 cobalt sulfate 7-water 0.015-0.017 chlorine tin 0.015-0.017 barium chloride 0.005-0.006 selenium 0.001-0.003,
high-temperature hydrolysis of the enriched suspension of hay is carried out at a temperature of 150-160 ° C and a pressure of 4.5-6 atm for 40-90 minutes, the formation of a biologically active preparation during evaporation occurs at a temperature of 60-120 ° C. 2. The method of obtaining a biologically active drug based on alfalfa hay according to claim 1, characterized in that at each stage of the recycling, a new portion of hay, water condensate and micro and macro elements is loaded into the steaming unit and the concentrated hydrolyzate is cleaned of waste, and the mass is again loaded hay, water condensate micro and macro elements is equivalent to the mass of waste. 3. The method of obtaining a biologically active preparation based on alfalfa hay according to claim 1, characterized in that when the concentration of nutrients is more than 5% in the concentrated hydrolyzate, part of the concentrated hydrolyzate is directed to evaporation, while an equivalent amount of aqueous condensate and micro - and macrocells.

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